Matters



UNITED "STATES PATENT much.

AUGUST BERNTHSEN, OF HEIDELBEBG, BADEN, ASSIGNOR TO THE BADISCHE ANILIN AND SODA. FABRIK, OF MANN HEIM, GERMANY.

SULPHURETED DERIVATIVE OF DIPHENYLAM INE AS A BASIS FOR THE PRODUCTION OF COLORING- MATTERS.

SPECIFICATION forming part of Letters Patent No. 286,526, dated October 9, 1883.

Application filed September 8, 1883.

sulphur as an essential element of their con-' stitution, of which the following is a specifition.

This invention relates to the production of thiodiphenylaminea new sulphureted derivative of diphenylamine, capable of being con- 1 5 vertedinto dye-stuffs or coloring-matters,forniing the subject-matter of Letters Patent No. 282,835, issued to me August 7, 1883.

In carrying out this invention, I submit diphenylamine to the action of sulphur in order to effect a substitution of sulphur for hydrogen.

As an example of the manner in which my invention may be carried into effect, I proceed as follows: About ten parts, by weight, of 2 5 diphenylamine are mixed with about four parts, by weight, of sulphur, and the mixture is heated in asuitable vessel or still provided with proper appliances for safely carrying off the sulphuret-ed hydrogen generated through 5 o outthe process. Iprefer to maintainthe temperature at about from 250 to 300 centigrade during two hours, or until the development of sulphureted hydrogen has ceased, or nearly so. In order to purify the crude thiodiphenylp 5 amine thus produced, I prefer to submit the same to fractional distillation, and the portion distilling above 350 centigrade may then be further purified by allowing its alcoholic solution to crystallize.

(No specimens.)

The characteristic properties of thiodiphe- 4o nylamine are as follows: It is a yellowish- White crystalline solid, soluble in alcohol, ether, benzine, glacial acetic acid, sparingly soluble in petroleum, naphtha, and insoluble in water. It readily dissolves in concentrated 5 sulphuric acid. According to the thickness of the layer, light is transmitted through the solution with a color varying from a greenislr black to a yellow or pink. The dilute alcoholic solution is colored intensely green on addition of perchloride of iron.

Thiodiphenylamine is readily acted upon by nitric acid in the cold, and the nitro-substitution product thus obtained, upon being submitted to the action of reducing agents 5 5 such as tin and hydrochloric acidis converted into a colorless base, which by oxidation assumes an intense purple coloration, owing to the production of a dyestnff, the preparation of which will be made the subject-matter of a separate application for Let ters Patent.

\VhatI claim as new, and desire to secure by Letters Patent, is

The within-described process forproducing a new sulphureted derivative of diphenylamine,which I call thiodiphenylamine, by heating diphenylamine with sulphur, and purifying the product thus obtained by distillation,-substantially in the manner herein set forth. y

In testimony whereof I have hereunto set my hand in the presence of two subscribing witnesses.

A. BERNTHSEN.

Witnesses:

Dr. T. CHAMBERS, J OHANNES Bii'rrNER. 

